Ma Yamin, Liu Haiyan, Wei Aile, Qin Junxiao, Zhang Shiqi, Zhang Wen, Bai Ligai
College of Pharmaceutical Sciences, Hebei University, Key Laboratory of Pharmaceutical Quality Control of Hebei Province, Baoding 071002, China.
Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education, Baoding 071002, China.
J Chromatogr Sci. 2016 Nov;54(10):1727-1734. doi: 10.1093/chromsci/bmw129. Epub 2016 Oct 11.
Poly(N-isopropylacrylamide-co-hexanediol diacrylate-co-ethylene dimethacrylate) [poly(NIPAAm-co-HDDA-co-EDMA)] monolithic column was prepared via in situ polymerization reaction. In order to investigate the porous properties of the monoliths prepared, the morphology was characterized by the scanning electron microscopy; the chemical group of the monolithic column was confirmed by a Fourier transform infrared spectroscopy method. The surface area was 39.1 m/g by the nitrogen adsorption-desorption experiment. With methanol as the mobile phase, the permeability of the monolithic column was calculated as 3.2330 × 10 m Then it was used as the stationary phase of high performance liquid chromatography. The results indicted that poly(NIPAAm-co-HDDA-co-EDMA) monolithic column was good to separate small molecules by controlling the temperature. Column efficiency for p-chloronitrobenzene was 4,680 plates/m. Repeatability was defined by determining run-to-run and column-to-column variation of the retention times of aromatic compounds, expressed as relative standard deviation (RSD = standard deviation/mean × 100%), and the values were <0.58% and 3.1%, respectively.
通过原位聚合反应制备了聚（N-异丙基丙烯酰胺-共-己二醇二丙烯酸酯-共-乙二醇二甲基丙烯酸酯）[聚（NIPAAm-共-HDDA-共-EDMA）]整体柱。为了研究所制备整体柱的多孔性能，通过扫描电子显微镜对其形态进行了表征；采用傅里叶变换红外光谱法确定了整体柱的化学基团。通过氮气吸附-脱附实验测得比表面积为39.1 m²/g。以甲醇为流动相，计算得到整体柱的渗透率为3.2330×10⁻⁶ m²。然后将其用作高效液相色谱的固定相。结果表明，聚（NIPAAm-共-HDDA-共-EDMA）整体柱通过控制温度对小分子具有良好的分离效果。对氯硝基苯的柱效为4680理论塔板数/米。通过测定芳香族化合物保留时间的批间和柱间变化来定义重复性，以相对标准偏差表示（RSD =标准偏差/平均值×100%），其值分别<0.58%和3.1%。
